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Sodium Hydroxide → HCID 58917331、化合物

HRID 547318
ノート
印刷プレビュー

反応式

HRID 547318 の反応式
[CH2:1]([O:3][CH2:4][C:5]1[N:6]([CH2:19][C:20]2([O:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:29])=[O:28])[CH2:23][CH2:22][CH2:21]2)[C:7]2[C:16]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[N:10]=[C:9]([NH2:17])[C:8]=2[N:18]=1)[CH3:2].[H][H].[OH-].[Na+]>FC(F)(F)C(O)=O.O.[Pt](=O)=O>[CH2:1]([O:3][CH2:4][C:5]1[N:6]([CH2:19][C:20]2([O:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:29])=[O:28])[CH2:21][CH2:22][CH2:23]2)[C:7]2[C:16]3[CH2:15][CH2:14][CH2:13][CH2:12][C:11]=3[N:10]=[C:9]([NH2:17])[C:8]=2[N:18]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 58917341HCID 58917341、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 58917331HCID 58917331、化合物収率 69.1%

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 962Water溶媒
HCID 6422
Trifluoroacetic acid
溶媒

実験手順

A mixture of 2-(ethoxymethyl)-1-({1-[2-(methylsulfonyl)ethoxy]cyclobutyl}methyl)-1H-imidazo[4,5-c]quinolin-4-amine (prepared as described in Example 26, 0.500 g, 1.16 mmol) and platinum(IV) oxide (0.5 g) in trifluoroacetic acid (5 mL) was hydrogenated on a Parr apparatus at 50 psi (3.5×105 Pa) hydrogen pressure for 1 day. The mixture was filtered through CELITE filter agent, which was washed afterwards with dichloromethane. The filtrate was concentrated under reduced pressure to afford an oil that was suspended in water (20 mL) and adjusted to pH 13 with 50% aqueous sodium hydroxide. A white solid formed that was isolated by filtration, washed with water, and recrystallized from acetonitrile. The crystals were isolated and dried under vacuum at 65° C. to afford 0.35 g of 2-(ethoxymethyl)-1-({1-[2-(methylsulfonyl)ethoxy]cyclobutyl}methyl)-6,7,8,9-tetrahydro-1H-imidazo[4,5-c]quinolin-4-amine as a white powder, mp 186-188° C.

後処理

  1. filtrationThe mixture was filtered through CELITE
  2. filtrationfilter agent, which
  3. washwas washed afterwards with dichloromethane
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customto afford an oil that
  6. customA white solid formed that
  7. customwas isolated by filtration
  8. washwashed with water
  9. customrecrystallized from acetonitrile
  10. customThe crystals were isolated
  11. customdried under vacuum at 65° C.

出典と根拠

ORDレコード
ord-5629d04b98164af58253436d82c8f3c5
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07939526B2

反応ノート

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